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  #1  
Old 06-09-2008, 04:21 PM
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Testing For Conversion

Hey all, to the board, http://www.ford-trucks.com/forums/74...say-hello.html

But I do have some first hand expeerience in to brewing of Bio. I know its not necessary, but I do have a laboratory background but its in Civil Engineering. I use and have access to different types of lab. equipment for running tests like; max maximum theoretical density, titration, hydrometer and so on (materials testing type stuff for Civil applications).

My question is;
  1. does any-one have ASTM's they would like to share for "Quality Testing"? Mainly to see if I have any of the lab equipment needed to perform the tests.
  2. Does any-one use the "27 & 3" Test? The one Utah Bio Supply uses for a first indicator of conversion?
So far, most of my small test batches (5 gal) processed & water washed, pass the "27 & 3" test, but I did have one that failed.

What should I do when I come across this again?

When it failed, I re-titrated and the titration was similar to that of clean SVO, if not less. I then re-processed a 1 litre batch of it with 20% methanol and 5.500 grams of KOH, as recomended by journeytoforever.org. This made a BAD emulsion, a batch that was so full of soap it was hard to wash and had a low yeild.
  • Next time, should I just keep washing before attempting a Re-Run?
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Old 06-09-2008, 04:33 PM
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8 grams is a better base for KOH. i found that out when I had a test batch emulsify. i use the 3/27 and the freezer test on my finished product.
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Old 06-09-2008, 06:05 PM
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Oh, BTW; My KOH is 89.6% pure.
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Old 06-09-2008, 06:08 PM
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Quote:
Originally Posted by empiretc View Post
8 grams is a better base for KOH. i found that out when I had a test batch emulsify. i use the 3/27 and the freezer test on my finished product.
empiretc, what do you do with your batch if it fails the 3/27?
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Old 06-09-2008, 06:27 PM
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reprocess it.
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Old 06-09-2008, 08:31 PM
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The first thing you'll need is a Gas Chromatograph, or a Ion Chromatograph ( I have both ) Neither is cheap............The cost to equip a Lab capable of doing ASTM biodiesel testing is about $250,000. Not many home-brewers can afford that.................
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Old 06-09-2008, 09:16 PM
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Quote:
Originally Posted by fabmandelux View Post
The first thing you'll need is a Gas Chromatograph, or a Ion Chromatograph ( I have both ) Neither is cheap............The cost to equip a Lab capable of doing ASTM biodiesel testing is about $250,000. Not many home-brewers can afford that.................
I do understand the cost associated with setting up a lab. and staff capable of passing AMRL & AASHTO accreditation (Not sure if Bio requires the same, I doubt it). I had set up a main lab and multiple portable labs in the past for Civil related designs. Your 100% correct, it big bucks!

I'm not looking to set up. To start, I'm more interested looking thru the apparatus portion of ASTM D658 to see if I have access to any of the lab equipment. I also have access to a full blown water quality lab that may or may not render the equipment .

Do you have at least the apparatus portion of D658 that you would be willing to share? You may be able to save me the 35 bones & alot of time

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Old 06-09-2008, 09:36 PM
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Originally Posted by empiretc View Post
reprocess it.
You belive I should of re-processed that batch with 8 grams for base KOH, even though I made a heavy emulsion with a re-process of 5.5grams? Should I still use 20% Methanol?

hmmm, I was thinking I over shot it with 5.5 the second time.

Is it feasible to just keep washing the first batch with out the re-process? Do you think I could still get a quality fuel with more washing?
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Old 06-09-2008, 10:42 PM
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I don't have all the test requirements, but I have some:
ASTM D130, Copper corrosion test
ASTM D445, Kinematic Viscosity
ASTM D1160 Vacuum Distillation
ASTM D 1796 Water and Sediment in Oils
ASTM D2500 Cloud Point
ASTM D6371 Wax Appearance Point
ASTM D14112 Oxidation Stabilty of Fatty Acid Methyl Esters (FAME)

And the biggie: ASTM D613 Cetane Number. This test requires a Cetane Test Engine.............About $65,000!

PLUS, an ICP-OES, IE: Inductively-Coupled Plasma-Optical Emission Spectroscopy.

Phydeaux 88 is our resident chemist here, he can probably supply the missing pieces.
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Old 06-10-2008, 12:57 AM
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Quote:
Originally Posted by Az.scarecrow View Post
You belive I should of re-processed that batch with 8 grams for base KOH, even though I made a heavy emulsion with a re-process of 5.5grams? Should I still use 20% Methanol?

hmmm, I was thinking I over shot it with 5.5 the second time.

Is it feasible to just keep washing the first batch with out the re-process? Do you think I could still get a quality fuel with more washing?
the batch that emulsified is trash. i was talking about a good looking batch that does not pass the 3/27 test.

you need to make sure you get all the glycerin out before you wash. this is why it is a good idea to take a small sample out and do a test wash on it before you attempt to wash the entire batch.

i have since switched to NaOH so i can make my own "roundup". it has gone up as well and the NaOH is a lot cheaper than KOH, so it just was a better choice. I will use 5g as base for that and I use ~25% methanol.
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Old 06-10-2008, 09:25 PM
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Quote:
Originally Posted by empiretc View Post
the batch that emulsified is trash. i was talking about a good looking batch that does not pass the 3/27 test.

you need to make sure you get all the glycerin out before you wash. this is why it is a good idea to take a small sample out and do a test wash on it before you attempt to wash the entire batch.

i have since switched to NaOH so i can make my own "roundup". it has gone up as well and the NaOH is a lot cheaper than KOH, so it just was a better choice. I will use 5g as base for that and I use ~25% methanol.
Hey empiretc, I think we may have a slight confusion of communication (sorry, that my be on me)
  • I made a 5 gal batch, washed it three times without trouble [on the left in the pic "dried"] (maybe 1/8" - 1/4" emulsion between the Bio & water in a 5 gal. water container), then I ran the 3/27.
  • The washed 5 gal. batch failed the 3/27.
  • I then pulled out 1 litre of the 5 gallon washed bio and re-processed the 1 litre washed bio with 5.5gr KOH @ 20% methanol.
  • This is when I got the bad emulsion. I had a define line between the bio and the emulsion, but the bottom was NASTY.9 (on the right in the pic) Is that considered a "bad reaction with heavy emulsion"? Thats the worst I have had since I started.

Here's a PIC

Click the image to open in full size.

More less my question is,
A) Do you think I over shot it when I added the 5.5gr of KOH the second time? Is to much lye what causes the the emulsion?

B) Should I have just continued washing the first 5 gal a few more times and run it as is in my truck?

Thanks for your patients with ME guys, I know I'm the Noobe .
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  #12  
Old 06-10-2008, 10:03 PM
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Quote:
Originally Posted by fabmandelux View Post
I don't have all the test requirements, but I have some:
ASTM D130, Copper corrosion test
ASTM D445, Kinematic Viscosity
ASTM D1160 Vacuum Distillation
ASTM D 1796 Water and Sediment in Oils
ASTM D2500 Cloud Point
ASTM D6371 Wax Appearance Point
ASTM D14112 Oxidation Stabilty of Fatty Acid Methyl Esters (FAME)

And the biggie: ASTM D613 Cetane Number. This test requires a Cetane Test Engine.............About $65,000!

PLUS, an ICP-OES, IE: Inductively-Coupled Plasma-Optical Emission Spectroscopy.

Phydeaux 88 is our resident chemist here, he can probably supply the missing pieces.
WOW fabmandelux! That's a completely different animal
I had never even heard of most that equipment.
I figured our asphalt (Bitumen) binder lab or one of the others would have something useful besides flasks, scales, thermometers and beakers

Oh, BTW; I didnt give you guys the correct ASTM I was looking for, I was interested in ASTM 6584-07. Do you have any info on the importance of this method compared to the others you listed?

Thanks,
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Old 06-10-2008, 10:03 PM
 
 
 
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